EP0100174A1 - Verfahren zur Herstellung einer optischen Faser - Google Patents

Verfahren zur Herstellung einer optischen Faser Download PDF

Info

Publication number
EP0100174A1
EP0100174A1 EP83304017A EP83304017A EP0100174A1 EP 0100174 A1 EP0100174 A1 EP 0100174A1 EP 83304017 A EP83304017 A EP 83304017A EP 83304017 A EP83304017 A EP 83304017A EP 0100174 A1 EP0100174 A1 EP 0100174A1
Authority
EP
European Patent Office
Prior art keywords
preform
aperture
mandrel
glass
soot
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP83304017A
Other languages
English (en)
French (fr)
Other versions
EP0100174B1 (de
Inventor
George Edward Berkey
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Corning Glass Works
Original Assignee
Corning Glass Works
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from US06/402,056 external-priority patent/US4453961A/en
Priority claimed from US06/427,525 external-priority patent/US4486212A/en
Application filed by Corning Glass Works filed Critical Corning Glass Works
Priority to AT83304017T priority Critical patent/ATE28177T1/de
Publication of EP0100174A1 publication Critical patent/EP0100174A1/de
Application granted granted Critical
Publication of EP0100174B1 publication Critical patent/EP0100174B1/de
Expired legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B35/00—Transporting of glass products during their manufacture, e.g. hot glass lenses, prisms
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/01486—Means for supporting, rotating or translating the preforms being formed, e.g. lathes
    • C03B37/01493—Deposition substrates, e.g. targets, mandrels, start rods or tubes
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/01466—Means for changing or stabilising the diameter or form of tubes or rods
    • C03B37/01473—Collapsing
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2203/00—Fibre product details, e.g. structure, shape
    • C03B2203/10—Internal structure or shape details
    • C03B2203/18—Axial perturbations, e.g. in refractive index or composition
    • C03B2203/20—Axial perturbations, e.g. in refractive index or composition helical

Definitions

  • the present invention relates to an improved method of forming a soot preform from which optical waveguide fibers can be made.
  • Certain glass making processes have been commonly employed in the formation of optical waveguide blanks.
  • a plurality of constituents in vapor form are entrained in a gaseous medium in predetermined amounts and thereafter are oxidized in a flame to form particulate glass called soot.
  • a first soot coating of uniform or radially varying composition is applied to the surface of a rotating cylindrical mandrel or starting member. After the first coating of soot is deposited to form the core glass, the composition of the soot is changed to form a cladding glass coating.
  • U.S. Patent No. 4,298,365 teaches a method which further facilitates the closing of the soot preform aperture during consolidation.
  • a thin stratum of very low viscosity glass soot is initially applied to the surface of a mandrel.
  • First and second coatings of glass soot are then deposited on the surface of the thin stratum in accordance with the teachings of the aforementioned Blankenship patent.
  • the mandrel is removed, and the soot preform is subjected to a high temperature whereby it is consolidated to form a dense glass blank.
  • the glass surface tension and the relative viscosities of the inner and outer portions of the preform cause the aperture to close during the consolidation process.
  • the thin stratum which may include P205 or B 2 0 3 smooths over the damage caused by removing the mandrel and reduces or even eliminates seed formation at the axis of the resultant glass blank.
  • Fibers having cores that are free from P 2 O 5 or B 2 0 3 eg. fibers having cores consisting of Ge0 2 -doped silica, are preferred for low-loss operation in the infrared region of the spectrum.
  • the aperture in a preform having a GeO 2 -SiO 2 core region does not close during consolidation.
  • the method of the present invention comprises applying at least one coating of particulate glass to the outside peripheral surface of an elongated mandrel.
  • the mandrel is removed to form a porous preform having a longitudinal aperture therethrough.
  • the porous preform is heated to form an elongated, consolidated glass preform having an aperture therethrough.
  • One end of the aperture is caused to close, the aperture is evacuated, and the other end is closed.
  • the resultant article can be immediately subjected to further processing or can be stored without risk of contaminating the walls of the aperture.
  • the consolidation step is preferably performed with a capillary tube at one end of the preform aperture.
  • a drying gas flowed into the aperture initially exhausts through the capillary tube. After the capilary tube closes due to the high consolidation temperature, the drying gas flows through the preform interstices. After consolidation, the closed end of the preform is severed to permit the etchant to flow freely through the aperture.
  • the etching step is followed by rinsing and drying.
  • the glass particles are deposited on the mandrel in such a manner as to. prevent the formation of a devitrified layer on the walls of the aperture during consolidation.
  • a porous preform is conventionally formed by directing a stream of glass particles toward the rotating mandrel, and reciprocatingly moving the stream longitudinally with respect to the mandrel. The combination of the rotation of the mandrel and the reciprocating movement of the stream with respect to the mandrel causes the stream to impinge upon the mandrel along a spiral path. Continued deposition of the particles causes a coating of uniform thickness to be built up on the mandrel.
  • the mandrel is removed to form a tubular porous glass preform which is consolidated to form a tubular glass article.
  • the first plurality of layers of glass particles are deposited on the surface of the-mandrel at a deposition rate that is sufficiently low that no spiral pattern of deposited glass particles is visible, whereby there is forme.d during the consolidation process a tubular glass article, the aperture-forming surface of which is free from devitrification.
  • the preform may be directly drawn into an optical fiber, ot-it may be drawn into a large diameter intermediate fiber upon which additional cladding material may be added.
  • the low pressure within the preform aperture with respect to that on the outer surface thereof assists the aperture closing process.
  • the drawings are illustrative and symbolic of the invention, and there is no intention to indicate scale or relative proportions of the elements shown therein.
  • the present invention expressly contemplates both single mode and multimode waveguides regardless of any specific description, drawing, or example set out herein.
  • the present invention also contemplates optical waveguides having cores with either a constant or gradient index of refraction.
  • the cladding may be the outer portion of the core, or it may be a layer whose refractive index is lower than that of the adjacent core material by such an amount that there is an abrupt change in refractive index at the core-cladding interface.
  • a porous preform may be formed in accordance with the method illustrated in Figures 1 and 2.
  • a handle 10 of the type disclosed in U.S. Patent No. 4,289,522 may be employed.
  • Handle 10 is a tubular member having a ground glass joint 12 at the one end thereof.
  • the large diameter end of a tapered mandrel 20 extends through handle 10 and is secured thereto by shims 18.
  • the ends of the mandrel are mounted in a lathe where it is rotated and translated as indicated by the arrows.
  • the mandrel may be provided with a layer of carbon soot to facilitate removal of the soot preform.
  • Fuel gas and oxygen or air are supplied to burner 24 from a source (not shown). This mixture is burned to produce a flame which is emitted from the burner. A gas-vapor mixture is oxidized within flame to form a soot stream 26 which is directed toward mandrel 20. Suitable means for delivering the gas-vapor mixture to the burner are well known in the art; for an illustration of such means reference is made to U.S. Patent Nos. 3,826,560, 4,148,621 and 4,173,305. One or more auxiliary burners (not shown) may be employed to direct a flame toward one or both ends of the soot preform during deposition to prevent breakage. This method can be employed to produce any type of core index profile including step index and gradient index.
  • Soot deposition means 24 may also comprise nozzles such as those disclosed in U.S. Patent No. 3,957,474 which emit reactant vapors which are heated by means such as a laser beam to form a soot stream.
  • FIG. 7 A fragmentary cross-sectional view of a conventional flame hydrolysis burner which may be employed as deposition means 24 is illustrated in Figure 7.
  • a centrally located orifice 76 in burner face 78 is surrounded by concentric rings of orifices 80, 82 and 84.
  • the reactant compounds emanate from orifice 76 where they are subjected to heat from a flame produced by the fuel gas and oxygen emanating from orifices 82.
  • a stream of oxygen, referred to as the inner shield emanates from orifices 80; this stream prevents reaction of the reactant compounds at the burner face.
  • a stream of oxygen referred to as the outer shield emanates from orifices 84.
  • This burner design is somewhat similar to that disclosed in U.S. Patent No.
  • the burner is generally operated under conditions that will provide acceptably high laydown rates and efficiency while minimizing the buildup of soot on face 78. Under such conditions, the flow rates of gases and reactants from orifices 76, 80, 82 and 84 and the sizes and locations of such orifices as well as the axial orientation thereof are such that a well focused stream of soot flows from the burner toward the mandrel.
  • a shield 86 which is spaced a short distance from face 78 by brackets 88, protects the soot stream from ambient air currents and improves laminar flow.
  • stratum 16 of silica soot may be initially deposited ' on the mandrel to create a compressive layer at the aperture forming surface of the resultant consolidated glass preform.
  • a coating 22 of glass soot is deposited on stratum 16.
  • a second coating 28 of soot may be applied over the outside peripheral surface of first coating 22 as shown in Figure 2.
  • Each of the coatings 22 and 28 is generally formed of a plurality of layers.
  • the refractive index of coating 28 is made lower than that of coating 22 by changing the composition of the soot being produced in flame 26. This can be accomplished by changing the concentration or type of dopant material being introduced into the flame, or by omitting the dopant material.
  • Mandrel 20 is again rotated and translated to provide a uniform deposition of coating 28.
  • the composite structure including first coating 22 and second coating 28 constitutes porous preform 30.
  • the materials of the core and cladding of the waveguide should be produced from a glass having minimum light attenuation characteristics, and although any optical quality glass may be used, fused silica is a particularly suitable glass.
  • fused silica is a particularly suitable glass.
  • the core glass may desirably be formed of the same type of glass used for the cladding and doped with a small amount of some other material to slightly increase the refractive index thereof.
  • the core glass can consist of fused silica doped with a material to increase its refractive index.
  • fused silica Many suitable materials have been used as a dopant alone or in combination with each other to increase the refractive index of fused silica. These include, but are not limited to, titanium oxide, tantalum oxide, aluminum oxide, lanthanum oxide, phosphorus oxide and germanium oxide.
  • a core of germania doped fused silica is advantageously employed as a fiber core material since the resultant fiber exhibits low loss characteristics which extend to around 1600 nm.
  • the cladding may be pure fused silica or silica doped with an oxide the amount of which is such that the cladding refractive index is lower than that of the core.
  • the cladding could be doped with an oxide such as boron oxide which provides a refractive index slightly lower than that of pure fused silica and also gives the cladding layer a somewhat higher thermal coefficient of expansion than pure fused silica, thereby providing a better match between the coefficients of expansion of the core and cladding materials.
  • an oxide such as boron oxide which provides a refractive index slightly lower than that of pure fused silica and also gives the cladding layer a somewhat higher thermal coefficient of expansion than pure fused silica, thereby providing a better match between the coefficients of expansion of the core and cladding materials.
  • mandrel 20 may be removed from the assembly by pulling it out through handle 10, thereby leaving a longitudinal aperture 32, as shown in Figure 3. Integral handle 10 provides a support for subsequent handling and processing.
  • Drying can be facilitated by inserting a short section 34 of capillary tubing into that end of the porous preform aperture 32 opposite handle 10 as shown in Figure 3.
  • the capillary tubing 34 initially permits some of the drying gas to flush water from_the central region of the preform.
  • the capillary tubing aperture closes, thereby causing all drying gas to thereafter flow through the preform interstices.
  • the aperture-forming surface of the consolidated preform may contain a devitrified layer.
  • the tendency for devitrification to occur is composition sensitive.
  • the deposition of pure silica stratum 16 results in a devitrified layer if that stratum is deposited under conventional conditions.
  • One embodiment of this invention which will be described in detail below, results in the formation of a fine, uniformly deposited stratum of pure silica which does not devitrify.
  • soot compositions such as silica
  • soot deposition techniques result in the formation of a devitrified layer on the aperture-forming surface of the consolidated glass preform.
  • the tendency for the aperture-forming surface to devitrify is initially manifested by the formation of a white spiral 90 on the mandrel surface as the soot is being deposited thereon as illustrated in Figure 8 by a dense dot pattern.
  • the spiral pattern is a manifestation of'a variation in the density of the deposited soot.
  • Spiral pattern 90 is formed along the spiral path along which the center of focused soot stream 26 is directed as mandrel 20 rotates and axially translates with respect to burner 24.
  • soot particles deposit with much lower density in those regions. It is thought that this variable density in the soot layer, which forms the surface of the preform aperture upon removal of the mandrel, causes devitrification sites which initiate devitrification during consolidation of the soot preform.
  • a consolidated preform is shown in Figure 4. After consolidation has occurred, the entire aperture-forming surface 42 of the preform has a white, frosty appearance while the remainder of the preform is transparent. If such a devitrified layer exists in the preform, a fiber drawn therefrom will contain seeds unless the layer is removed from the aperture-forming surface prior to the time that the aperture is closed.
  • the aperture surface is preferably etched to remove the devitrified layer, and thereafter rinsed and dried before the aperture is sealed. If a capillary tube has sealed the end of the aperture during consolidation, the sealed end 44 should be severed prior to etching. After the sealed end has been severed, aperture 42 extends through the entire preform and handle.
  • the rinsing fluid and the drying gas are flowed through the aperture, that portion of the aperture at preform end 44 is again closed, the aperture is evacuated, and the other end 48 is heated and closed.
  • the exposed aperture surface can be contaminated by OH-ions or other absorption impurities which can diffuse into the aperture-forming surface while it is subjected to high temperature during drawing. Since aperture 42 is evacuated and closed, it cannot be contaminated in this manner.
  • the aperture forming surface 42 may not need to be etched. It is thought that the surface of aperture 42 would not devitrify during consolidation if the composition of stratum 16 was 15 wt. % P 2 O 5 , 6 wt. % GeO 2 and 79 wt. % Si0 2 .
  • the composition of coating 22 could be 10 wt. % Ge0 2 , 90 wt. % Si0 2 and that of cladding coatings 28 and 70 pure Si0 2 . If these compositions were employed, aperture 42 would remain open. Thus, if end 44 of preform aperture 42 closes during consolidation, as shown in Figure 4, it can remain closed . If no plug 34 is employed, the entire aperture will remain open. In this event end 44 must be closed after consolidation by a technique such as heating and pinching the same. The aperture is then evacuated through handle 10, and the other end 48 is heated and closed.
  • devitrification of the surface of the preform aperture is prevented even though there is deposited a soot composition which would devitrify if deposited under conventional conditions.
  • the first plurality of layers of glass soot is deposited on the mandrel at a deposition rate that is sufficiently low that no spiral pattern of deposited soot is visible.
  • a layer is defined as that portion. of a glass soot preform that is formed by the soot which is deposited by one pass of the burner along the mandrel.
  • the method of this embodiment is illustrated in Figure 9 wherein the first pass of burner 24 along mandrel 20 results in the deposition of a layer 94 of soot which is so fine that hardly any glass soot can be seen. After many layers are deposited, the fine soot stratum becomes continuous. Although more than 50 burner passes were actually employed in the deposition of the fine soot layer in the example described hereinbelow, the actual number of passes could deviate widely from that number without departing from the scope of the invention. For example, the initially deposited fine soot stratum can be made much thicker than the minimum thickness required to prevent devitrification, but this would decrease the amount of glass deposited per unit time and thus increase cost of production. If the deposition of the fine soot stratum is not continued for a time sufficient to render it continuous, the application of conventionally applied soot coatings on the discontinuous stratum may still result in devitrification.
  • Deposition of a fine, spiral-free coating 94 has been achieved by supplying the burner with a greatly reduced flow of reactant vapors.
  • the absence of a high velocity reactant vapor stream emanating from orifice 76 tends to generate a defocused soot stream 96 that is incapable of depositing a coating of soot having a sufficient density variation to appear as a spiral.
  • a focused soot stream 98 can be directed above or preferably below the mandrel 20 as illustrated in Figure 10.
  • the major portion of soot stream 98 flows past the mandrel and is collected by exhaust hood 100. Just the soot at the edge of the focused stream impinges upon the mandrel. Buoyant effects cause more of the soot particles to depart upwardly from the focused stream.
  • the focused soot stream can be directed toward the mandrel for efficient deposition of the remainder of the preform.
  • FIG. 11 Another technique for depositing a fine soot stratum employs a burner of the type illustrated in Figure 11 wherein elements similar to those of Figure 7 are represented by primed reference numerals.
  • the axis of each of the orifices 80', 82' and 84' makes an angle with the axis of orifice 76'. Since the streams issuing from orifices 80', 82' and 84' diverge from that issuing from orifice 76', a diffuse soot stream is produced by the burner of Figure 11. After the unfocused soot stream is employed for a sufficient time to build up a continuous layer, a conventional burner such as that illustrated in Figure 7 is employed to efficiently deposit the remainder of the preform.
  • the aperture-forming surface of the consolidated preform does not devitrify.
  • Certain soot compositions have a tendency to devitrify when conventionally deposited, but devitrification can be avoided by depositing the first plurality of soot layers at a rate that is sufficiently low that no spiral pattern of deposited soot is visible. If devitrification does occur at the aperture-forming surface, it can be removwed by etching. Regardless of which of these techniques is employed, there results a consolidated preform having a devitrification-free aperture-forming surface that is also free of other contamination.
  • the aperture of the consolidated preform will be closed at end 44 as shown in Figure 4 if a capillary plug has been employed. If no plug has been employed the entire aperture will remain open. In thisjevent end 44 is closed after consolidation by a technique such as heating and pinching the same. The aperture is then evacuated through handle 10, and the other end 48 is heated and closed. The resultant article can be stored while awaiting further processing without risk of contaminating the aperture-forming wall.
  • the resultant consolidated preform is drawn directly into an optical waveguide fiber, the low pressure within the aperture will assist in the closing thereof.
  • the resultant preform may be provided with additional cladding material prior to drawing the optical waveguide fiber.
  • additional cladding material may be added by a flame oxidation process as taught in U.S. Patent No. 3,775,075 or the consolidated preform may be inserted into a tube of cladding material, the composite being drawn into an optical waveguide fiber. If additional cladding is to be provided, it is preferred that the consolidated preform be first drawn into an intermediate, large diameter fiber which is thereafter provided with additional cladding.
  • the intermediate fiber can be formed in a conventional draw furnace wherein the tip ot" the consolidated preform from which the intermediate fiber is being drawn is heated to a temperature which is slightly lower than the temperature to which the preform would be subjected to draw optical fiber therefrom.
  • a temperature of about 1900°C is suitable for a high silica content preform.
  • a suitable method for forming an intermediate fiber is illustrated in Figure 5.
  • Preform 40 is mounted in a conventional draw furnace where the tip thereof is heated by_ resistance heater 52.
  • a glass rod 54 may be attached to the bottom of preform 40.
  • a cord 60 is tied to rod 54.
  • Cord 60 is wound upon a motor-driven capstan 62, thereby causing the intermediate fiber 56 to be drawn at a suitable rate, a rate of 15 to 23 cm/min having been found to be adequate.
  • the aperture readily closes since the pressure therein is low relative to ambient pressure.
  • the aperture may close somewhat flat whereby the core roundness of the resultant fiber may be adversely affected.
  • the core of resultant fiber will not be unacceptably out of round if the core-clad ratio of intermediate fiber 56 is sufficiently high and if the intermediate fiber is employed as the central region upon which additional cladding is added in the formation of a single-mode or a multimode fiber.
  • the diameter of an intermediate fiber that is to be employed as a mandrel upon which cladding soot is to be deposited is preferably in the range of 4 to 10 mm. It is noted that core roundness should be satisfactory even if the preform 40 is drawn directly into an optical fiber, provided that the core-clad diameter ratio of the resultant fiber is sufficiently high.
  • That aspect of the invention whereby the final draw blank is formed in a two-step process involving the formation of an intermediate fiber results in less tensile stress in the inner core region of the consolidated preform.
  • the ratio of the core diameter to cladding diameter in preform 40 is larger than the value necessary to achieve the desired core diameter in the resultant fiber.
  • intermediate fiber 56 which comprises core region 66 and cladding region 68, is employed as a starting member upon which coating 70 is deposited by burner 72.
  • Coating 70 is generally formed of the same material as the cladding portion 68 of intermediate fiber 56.
  • the resultant composite preform 74 is preferably consolidated to form a solid glass draw blank which is thereafter drawn into an optical fiber.
  • composite preform 74 is gradually inserted into a furnace through which a consolidation atmosphere flows.
  • the atmosphere preferable contains helium and an amount of chlorine sufficent to dry the soot prior to the time that consolidation occurs. About 5 vol. % chlorine is usually sufficient. If chlorine is not used during this consolidation process, relatively high attenuation will be evident at 950 nm and 1400 nm.
  • An integral handle of the type disclosed in U.S. Patent No. 4,289,522 was employed.
  • a tapered alumina mandrel was inserted into the handle, the central region where soot particles were ultimately deposited being tapered from.about 5.5 mm to 6.5 mm.
  • the burner was located 13.7 cm from the mandrel.
  • Liquid SiCl 4 and liquid GeCl was maintained at 37°C in first and second containers, respectively.
  • the burner traversed a 49 cm section of mandrel in 25 seconds.
  • An acetylene torch supported on the burner was first employed to deposit carbon particles on the mandrel during three burner passes.
  • Silica soot having a thickness of about 1 mm was then deposited on the mandrel during fiber burner passes during which time oxygen flowed through the first container at a rate of 1.4 slpm. During the next 58 minutes oxygen was bubbled through the second container at a rate of 0.3 slpm while the flow rate of oxygen to the first container remained unchanged. Thus, a step-index core region of Si0 2 doped with 10 weight percent GeO 2 was deposited to a thickness of about 12 mm.
  • the soot preform was removed from the lathe, and the mandrel was removed therefrom, the integral handle remaining at one end thereof.
  • a short section of capillary tubing was inserted into that end of the preform aperture opposite the handle.
  • the preform was then simultaneously dried and consolidated in accordance with the teachings of U.S. Patent No. 4,125,388.
  • a drying gas consisting of 5 volume percent chlorine, the balance being helium, was flowed through the handle and into the preform aperture. A portion of this drying gas initially flowed through the capillary plug carrying with it water vapor along with reaction products from the drying reaction.
  • As the preform was lowered into the consolidation furnace, through which a helium flushing gas was flowing, the opening in the capillary tube became sealed, and the preform was subjected to gradient consolidation.
  • the tip containing the capillary plug was removed so that the aperture extended entirely through the preform.
  • the preform was then acid etched for 4 hours in a 50% HF bath which was maintained at 23°C. During this time it was repeatedly immersed and removed from the bath. During this etching step, a very thin layer of devitrified SiO 2 was removed from the aperture-forming surface of the preform.
  • the preform was then rinsed in filtered, deionized water and was permitted to dry at room temperature. Since some water remained on the aperture-forming surface, a drying gas mixture comprising 5 volume percent chlorine and 95 volume percent helium was supplied to the handle at about 1.5 psi and was flowed through the aperture.
  • the consolidated preform was then -immediately inserted into a lathe and a torch was directed at the end thereof opposite the handle.
  • the softened glass was then pinched to close the aperture at region 44.
  • the aperture was then evacuated through the handle. When the flame from a small torch was directed at the central region of the handle portion the aperture was quickly drawn shut to form pinched region 48.
  • the preform was then inserted into a draw furnace, and a cord was attached thereto.
  • the bottom tip of the preform was heated to about 1900°C while the cord pulled downwardly on the preform at a rate of about 15 cm/min.
  • the diameter of the resultant .intermediate fiber was about 5 mm.
  • the intermediate fiber had been drawn to a length of about 3 m, it was broken from the preform and severed into sections about 89 cm long.
  • the cord was reattached to the bottom of the undrawn portion of the preform, and the remainder of the preform was drawn into intermediate fiber.
  • Each of the sections of intermediate fiber was then subjected to the following steps.
  • a section of intermediate fiber was supported in the lathe where it functioned as a mandrel for the deposition of cladding soot.
  • Oxygen flowed through the first container at a rate of 1.6 slpm, and the burner traversed the intermediate fiber at a rate of about 2 cm/sec. This was continued until a layer of Si0 2 having an outside diameter of 60 mm was deposited.
  • the resultant final preform was gradually inserted into a consolidation furnace having a maximum temperature of 1450°C where it was consolidated while helium flowed upwardly through the furnace.
  • the resultant optical waveguide preform the diameter of which was about 35 mm, was inserted into the draw furnace where the tip thereof was subjected- to a temperature of about 2100°C.
  • the resultant step-index, single-mode optical waveguide fiber had a core diameter of about 8 ⁇ m and an outside diameter of 125 pm.
  • the spectral attenuation curve for this fiber is shown in Figure 12. The peaks at about 950 nm and 1400 nm are, indicative of a water content of about 3 ppm.
  • This example pertains to that embodiment wherein the initially formed layers of silica soot are deposited in such a manner that no devitrification appears at the aperture-forming surface of the consolidated preform.
  • Example 1 Unless otherwise specified, the details of this example are the same as those of Example 1.
  • a burner of the type illustrated in Figure 7 was located 13.7 cm from the mandrel.
  • oxygen flowed from inner shield orifices 80 and outer shield orifices 84 at 2.5 slpm and 3.0 slpm, respectively.
  • methane and oxygen flowed from orifices 82 at 6.5 slpm and 5.2 slpm, respectively.
  • the flow of methane and oxygen from orifices 82 was 5.8 slpm and 4.1 slpm, respectively.
  • An acetylene torch supported on the burner was first employed to deposit carbon particles on the mandrel during one burner pass.
  • Silica soot was then deposited on the mandrel for thirty minutes during which time oxygen flowed through the first container at a rate of 0.05 slpm to form a layer of low expansion silica soot having a thickness of about 1 mm.
  • the consolidated preform was then inserted into a lathe and the aperture was evacuated through the handle.
  • the aperture was quickly drawn shut to form pinched region 48.
  • the preform was drawn to an intermediate fiber which was severed into sections, each of which were coated with silica soot in accordance with Example 1.
  • the resultant final preform was consolidated and drawn into a fiber having a core diameter of about 8 pm.
  • the spectral attenuation curve for this fiber is shown in Figure 13.
  • the peaks at about 950 nm and 1400 nm are indicative of a water content of about 3 ppm.
  • the attenuation at 1480 nm is shown to be less than 0.1 dB/km.
  • the oxygen carrier flow rate for preform No. 3 was set at the level of 1.44 lpm, which is in the range of conventional flow rates for achieving efficient deposition of soot. Thereafter coatings 22 and 28 of core and cladding soot were applied as described above. After the resultant preform was consolidated, devitrification manifested by a frosty appearance was evident along the entire length of the aperture.
  • the carrier gas flow rate to the SiCl 4 reservoir was 0.2 1pm while stratum 16 was being deposited. After depositing coatings 22 and 28 and consolidating the resultant soot preform, a pattern of devitrification spirals were evident along the length of the blank.
  • the oxygen carrier gas flow rate for preform No. 5 was set at 0.1 lpm during the deposition of stratum 16. Thereafter, coatings 22 and 28 were deposited and the soot preform was consolidated. Most of the resultant consolidated preform was acceptable for the formation of optical waveguide fibers since there was no evidence of devitrification spirals along the aperture-forming surface. However, the .end of the aperture-forming surface opposite the handle contained a layer of devitrified glass. This portion of the preform would have to be removed prior to further processing.
  • preform No. 6 the flow rate of carrier gas to the SiCl 4 reservoir was 0.02 lpm during the formation of stratum 16. After depositing coatings 22 and 28 and consolidating the resultant soot preform, there was no evidence of devitrification on the aperture-forming surface of the preform. Thus, the entire preform would be suitable for the formation of optical waveguide fibers.
  • the soot flow rate was reduced during the deposition of the entire silica ' compressive stratum 16.
  • the soot flow rate could be reduced during the deposition of only the first plurality of layers of silica stratum 16, provided that the thickness of that initially formed portion is sufficient to prevent .
  • the occurrence of devitrification that is, provided that a continuous coating is formed by the first plurality of layers of fine soot.
  • the effect of the fine soot stratum i.e. the elimination of devitrification at the aperture-forming surface of the consolidated preform, is not limited to SiO 2 coatings.
  • Strata of silica doped with 15 wt. % GeO 2 as well as pure silica have both been effective in preventing devitrification. If either of these soot compositions were deposited at normal rates, devitrification would occur during consolidation.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture, Treatment Of Glass Fibers (AREA)
  • Glass Melting And Manufacturing (AREA)
  • Glass Compositions (AREA)
EP83304017A 1982-07-26 1983-07-11 Verfahren zur Herstellung einer optischen Faser Expired EP0100174B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT83304017T ATE28177T1 (de) 1982-07-26 1983-07-11 Verfahren zur herstellung einer optischen faser.

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US402056 1982-07-26
US06/402,056 US4453961A (en) 1982-07-26 1982-07-26 Method of making glass optical fiber
US06/427,525 US4486212A (en) 1982-09-29 1982-09-29 Devitrification resistant flame hydrolysis process
US427525 1982-09-29

Publications (2)

Publication Number Publication Date
EP0100174A1 true EP0100174A1 (de) 1984-02-08
EP0100174B1 EP0100174B1 (de) 1987-07-08

Family

ID=27017699

Family Applications (1)

Application Number Title Priority Date Filing Date
EP83304017A Expired EP0100174B1 (de) 1982-07-26 1983-07-11 Verfahren zur Herstellung einer optischen Faser

Country Status (11)

Country Link
EP (1) EP0100174B1 (de)
JP (1) JPH064491B2 (de)
KR (1) KR900004381B1 (de)
AU (1) AU560536B2 (de)
BR (1) BR8302985A (de)
CA (1) CA1187291A (de)
DE (1) DE3372358D1 (de)
DK (1) DK159875C (de)
FI (1) FI73405C (de)
MX (1) MX158461A (de)
NO (1) NO155487C (de)

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0163072A2 (de) * 1984-05-26 1985-12-04 AEG KABEL Aktiengesellschaft Verfahren zum Herstellen einer Vorform zum Ziehen von Lichtleitfasern
EP0163071A2 (de) * 1984-05-26 1985-12-04 AEG KABEL Aktiengesellschaft Verfahren zum Herstellen einer Vorform zum Ziehen von Lichtleitfasern
EP0251312A2 (de) * 1986-07-03 1988-01-07 Sumitomo Electric Industries Limited Verfahren zur Herstellung einer Faservorform für Einzelmodefasern
EP0367871A1 (de) * 1987-08-05 1990-05-16 Corning Glass Works Verfahren zum Herstellen einer Vorform für optische Fasern
EP0484659A2 (de) * 1990-11-09 1992-05-13 Corning Incorporated Verfahren zur Herstellung einer polarisationserhaltenden Faser
US5429653A (en) * 1991-05-31 1995-07-04 Heraeus Quarzglas Gmbh Method of partially introverting a multiple layer tube to form an optical fiber preform
EP0744383A1 (de) * 1995-05-22 1996-11-27 Corning Incorporated Verfahren zum Trocknen und Sintern einer Vorform für optische Fasern
WO2000064825A1 (en) * 1999-04-26 2000-11-02 Corning Incorporated Low water peak optical waveguide fiber and method of manufacturing same
EP1112233A1 (de) * 1998-05-29 2001-07-04 Corning Incorporated Verfahren zur herstellung einer glasvorform
WO2002036510A2 (en) * 2000-11-01 2002-05-10 Corning Incorporated Method of manufacturing an optical fiber preform
DE10112624B4 (de) * 2000-03-14 2007-03-29 Heraeus Tenevo Gmbh Verfahren zur Herstellung einer Vorform für optische Fasern und Verwendung eines Abscheidebrenners für diesen Zweck

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5678467B2 (ja) * 2010-04-30 2015-03-04 住友電気工業株式会社 ガラス母材製造方法
JP5533205B2 (ja) * 2010-04-30 2014-06-25 住友電気工業株式会社 ガラス母材製造方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4286978A (en) * 1980-07-03 1981-09-01 Corning Glass Works Method for substantially continuously drying, consolidating and drawing an optical waveguide preform
EP0041397A1 (de) * 1980-06-02 1981-12-09 Corning Glass Works Verfahren und Vorrichtung zum Herstellen einer Vorform für optische Wellenleiter sowie ein optischer Wellenleiter
GB2081250A (en) * 1980-07-31 1982-02-17 Boscher Daniel Method and apparatus for fabricating optical fibres

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS53162152U (de) * 1977-05-26 1978-12-19
JPS5414753U (de) * 1977-07-04 1979-01-30
JPS5516980A (en) * 1978-07-25 1980-02-06 Unitika Ltd Production of raised finished yarn
JPS5650130A (en) * 1979-09-27 1981-05-07 Sumitomo Electric Ind Ltd Manufacture of preform for optical transmission

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0041397A1 (de) * 1980-06-02 1981-12-09 Corning Glass Works Verfahren und Vorrichtung zum Herstellen einer Vorform für optische Wellenleiter sowie ein optischer Wellenleiter
US4286978A (en) * 1980-07-03 1981-09-01 Corning Glass Works Method for substantially continuously drying, consolidating and drawing an optical waveguide preform
GB2081250A (en) * 1980-07-31 1982-02-17 Boscher Daniel Method and apparatus for fabricating optical fibres

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0163072A2 (de) * 1984-05-26 1985-12-04 AEG KABEL Aktiengesellschaft Verfahren zum Herstellen einer Vorform zum Ziehen von Lichtleitfasern
EP0163071A2 (de) * 1984-05-26 1985-12-04 AEG KABEL Aktiengesellschaft Verfahren zum Herstellen einer Vorform zum Ziehen von Lichtleitfasern
EP0163071A3 (en) * 1984-05-26 1986-11-12 Aeg Kabel Aktiengesellschaft Method for producing a preform for drawing optical fibers
EP0163072A3 (en) * 1984-05-26 1986-12-10 Aeg Kabel Aktiengesellschaft Method for producing a preform for drawing optical fibers
EP0251312A2 (de) * 1986-07-03 1988-01-07 Sumitomo Electric Industries Limited Verfahren zur Herstellung einer Faservorform für Einzelmodefasern
EP0251312A3 (en) * 1986-07-03 1989-02-01 Sumitomo Electric Industries Limited Method of manufacturing fiber preform for single-mode fibers
EP0367871A1 (de) * 1987-08-05 1990-05-16 Corning Glass Works Verfahren zum Herstellen einer Vorform für optische Fasern
EP0738691A2 (de) * 1990-11-09 1996-10-23 Corning Incorporated Verfahren zur Herstellung eines länglichen Glaskörpers
EP0484659A3 (en) * 1990-11-09 1993-04-07 Corning Incorporated Method of making polarization retaining fiber
EP0484659A2 (de) * 1990-11-09 1992-05-13 Corning Incorporated Verfahren zur Herstellung einer polarisationserhaltenden Faser
EP0738691A3 (de) * 1990-11-09 1997-03-19 Corning Inc Verfahren zur Herstellung eines länglichen Glaskörpers
US5429653A (en) * 1991-05-31 1995-07-04 Heraeus Quarzglas Gmbh Method of partially introverting a multiple layer tube to form an optical fiber preform
EP0744383A1 (de) * 1995-05-22 1996-11-27 Corning Incorporated Verfahren zum Trocknen und Sintern einer Vorform für optische Fasern
EP1112233A1 (de) * 1998-05-29 2001-07-04 Corning Incorporated Verfahren zur herstellung einer glasvorform
EP1112233A4 (de) * 1998-05-29 2005-03-09 Corning Inc Verfahren zur herstellung einer glasvorform
WO2000064825A1 (en) * 1999-04-26 2000-11-02 Corning Incorporated Low water peak optical waveguide fiber and method of manufacturing same
US6477305B1 (en) 1999-04-26 2002-11-05 Corning Incorporated Low water peak optical waveguide and method of manufacturing same
DE10112624B4 (de) * 2000-03-14 2007-03-29 Heraeus Tenevo Gmbh Verfahren zur Herstellung einer Vorform für optische Fasern und Verwendung eines Abscheidebrenners für diesen Zweck
WO2002036510A2 (en) * 2000-11-01 2002-05-10 Corning Incorporated Method of manufacturing an optical fiber preform
WO2002036510A3 (en) * 2000-11-01 2002-07-11 Corning Inc Method of manufacturing an optical fiber preform

Also Published As

Publication number Publication date
NO155487C (no) 1987-04-08
KR840005418A (ko) 1984-11-12
MX158461A (es) 1989-02-02
NO832708L (no) 1984-01-27
FI832652A (fi) 1984-01-27
FI73405B (fi) 1987-06-30
JPH064491B2 (ja) 1994-01-19
JPS5939742A (ja) 1984-03-05
KR900004381B1 (ko) 1990-06-23
DK159875C (da) 1991-05-21
FI832652A0 (fi) 1983-07-21
AU1720483A (en) 1984-02-02
DK339183A (da) 1984-01-27
DK339183D0 (da) 1983-07-25
FI73405C (fi) 1987-10-09
AU560536B2 (en) 1987-04-09
NO155487B (no) 1986-12-29
CA1187291A (en) 1985-05-21
BR8302985A (pt) 1984-04-17
EP0100174B1 (de) 1987-07-08
DK159875B (da) 1990-12-24
DE3372358D1 (en) 1987-08-13

Similar Documents

Publication Publication Date Title
US4486212A (en) Devitrification resistant flame hydrolysis process
US4453961A (en) Method of making glass optical fiber
EP0139348B1 (de) Optische Faser und Verfahren zu deren Herstellung
US4157906A (en) Method of drawing glass optical waveguides
US4251251A (en) Method of making optical devices
US4413882A (en) Low viscosity core glass optical fiber
EP0484659B1 (de) Verfahren zur Herstellung einer polarisationserhaltenden Faser
US6422042B1 (en) Rit method of making optical fiber having depressed index core region
EP0522229B1 (de) Verfahren zum Herstellen einer polarisationserhaltenden, optischen Monomodenfaser
EP0147225A2 (de) Verfahren zum Herstellen einer optischen Faser
US6189342B1 (en) Method of making segmented core optical waveguide preforms
US4578097A (en) Method of forming a polarization preserving optical waveguide
US4298365A (en) Method of making a soot preform compositional profile
US5180410A (en) Method of making polarization retaining fiber
WO2004109352A1 (en) Optical fiber having reduced viscosity mismatch
EP0198510A1 (de) Verfahren zum Herstellen einer Glasvorform für optische Fasern
EP0100174B1 (de) Verfahren zur Herstellung einer optischen Faser
US4784465A (en) Method of making glass optical fiber
GB1596088A (en) Method of making glass articles

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Designated state(s): AT BE CH DE FR GB IT LI NL SE

17P Request for examination filed

Effective date: 19840712

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE CH DE FR GB IT LI NL SE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Effective date: 19870708

Ref country code: CH

Effective date: 19870708

Ref country code: BE

Effective date: 19870708

Ref country code: AT

Effective date: 19870708

REF Corresponds to:

Ref document number: 28177

Country of ref document: AT

Date of ref document: 19870715

Kind code of ref document: T

REF Corresponds to:

Ref document number: 3372358

Country of ref document: DE

Date of ref document: 19870813

ITF It: translation for a ep patent filed

Owner name: ING. A. GIAMBROCONO & C. S.R.L.

ET Fr: translation filed
REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed
ITTA It: last paid annual fee
PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SE

Payment date: 19940621

Year of fee payment: 12

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: NL

Payment date: 19940731

Year of fee payment: 12

EAL Se: european patent in force in sweden

Ref document number: 83304017.3

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Effective date: 19950712

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Effective date: 19960201

NLV4 Nl: lapsed or anulled due to non-payment of the annual fee

Effective date: 19960201

EUG Se: european patent has lapsed

Ref document number: 83304017.3

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 19960715

Year of fee payment: 14

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19980331

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20010614

Year of fee payment: 19

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20010731

Year of fee payment: 19

REG Reference to a national code

Ref country code: GB

Ref legal event code: IF02

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20020711

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20030201

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20020711